Flaxseed oil and hemp seed oil blended compound blend oil and preparation method thereof

文档序号:261830 发布日期:2021-11-19 浏览:11次 中文

阅读说明:本技术 一种亚麻籽油、火麻籽油调复配调和油及其制备方法 (Flaxseed oil and hemp seed oil blended compound blend oil and preparation method thereof ) 是由 王振 李素玲 许光映 高忠东 李群 车星星 田歌 毛恺 赵鑫 初玲玲 于 2021-08-23 设计创作,主要内容包括:本发明公开了一种亚麻籽油、火麻籽油调复配调和油及其制备方法,各组分原料如下,为亚麻籽、火麻籽、五倍子粉末、三聚磷酸钠。本发明亚麻籽中主要含有不饱和脂肪酸、蛋白质和矿物组,其中不饱和脂肪酸作为主要的营养成分能够调节血脂、清理血栓,可以参与免疫调节增强免疫力等作用,本发明加入了抗氧化剂丁基羟基茴香醚和三聚磷酸钠,它们可以作为抗氧化剂进行协同作用,增加产品的抗氧化能力,减少反式脂肪酸的产生,增加产品的保质期和营养成分的含量,将五味子进行萃取,将其中的鞣质提取出来,不仅能够增加产品的营养种类,还能够提高产品中不饱和脂肪酸的抗氧化能力的效果。(The invention discloses flaxseed oil and hemp seed oil blended and compounded blend oil and a preparation method thereof. The linseed mainly contains unsaturated fatty acid, protein and mineral group, wherein the unsaturated fatty acid can be used as a main nutrient component to regulate blood fat and clear thrombus and can participate in the functions of immunoregulation, immunity enhancement and the like.)

1. A flaxseed oil and hemp seed oil blended compound blend oil is characterized in that: the compound blend oil comprises the following raw materials, by weight, 5-10 parts of flaxseed, 15-30 parts of hemp seed, 3-5 parts of nutgall powder and 0.4-0.5 part of sodium tripolyphosphate.

2. A preparation method of flaxseed oil and hemp seed oil blended compound blend oil is characterized by comprising the following steps of: the steps are as follows,

(1) extracting Chinese gall powder:

adding deionized water into nutgall powder for leaching, filtering, decoloring, adding a solvent, heating at the temperature of 40-50 ℃, stirring for 30-40 min, standing for layering to obtain a tannin extracting solution and a supernatant;

secondly, taking out the supernatant obtained in the first step, adding sulfuric acid at the temperature of 90-95 ℃, stirring for 30-40 min, adding diethyl ether and ethyl acetate, stirring, standing and layering to obtain a supernatant A and a supernatant A;

taking out the supernatant A obtained in the second step, drying, adding deionized water at the temperature of 70-80 ℃ for dissolving, and adding glucose hydrolase and catalase to obtain a gluconic acid extracting solution;

adding propanol and sulfuric acid into the supernate A obtained in the step two, stirring, filtering after complete reaction, adding ethanol for extraction, extracting for 3 times, centrifuging, and heating to obtain propyl gallate extracting solution;

(2) preparing flaxseed and hemp seed oil:

heating 1/3 sodium tripolyphosphate, adding citric acid to obtain buffer solution, dehulling semen Lini, adding buffer solution, stirring, and hot pressing to obtain oleum Lini and residue A;

peeling hemp seeds, crushing, putting into an extraction tank, and performing subcritical butane extraction to obtain hemp seed oil and residue B;

mixing the residue A and the residue B, adding a tannin extracting solution, a gluconic acid extracting solution and a propyl gallate extracting solution, and extracting to obtain recovered nutritional ingredients;

and fourthly, mixing the linseed oil obtained in the step one and the hemp seed oil obtained in the step two, adding 2/3 sodium tripolyphosphate, stirring, adding the recovered nutritional ingredients obtained in the step three, mixing, stirring, centrifuging, decoloring and deodorizing, adding citric acid and butyl hydroxy anisole, heating, and removing organic solvents and enzymes to obtain the compound blend oil.

3. The preparation method of the flaxseed oil and hemp seed oil blended blend oil according to claim 2, characterized in that: the steps of recovering residue a and residue B are as follows,

mixing the residue A and the residue B, adding ethanol and a tannin extracting solution, heating in a water bath at the temperature of 80-90 ℃, adding sodium hydroxide, extracting for 1-2 hours, and centrifuging to obtain a supernatant;

adding a gluconic acid extracting solution and a propyl gallate extracting solution into the supernatant obtained in the step one, adding sodium hydroxide, maintaining the pH value at 6-7, stirring, standing, adding ethanol, stirring, cooling, wherein the temperature is 3-5 ℃, and centrifuging to obtain recovered protein and waste liquid;

thirdly, adding barium chloride into the waste liquid, stirring, filtering, heating and drying, adding ethanol, stirring, filtering, drying, repeating for three times to obtain recovered protein, and mixing with the recovered protein obtained in the second step to obtain recovered nutrient components.

4. The preparation method of the flaxseed oil and hemp seed oil blended blend oil according to claim 2, characterized in that: when the hemp seeds are extracted, the pressure of an extraction tank is controlled to be-0.1 to-0.05 MPa, the extraction temperature is 60 to 70 ℃, the butane flow is 2 to 3L/min, and the extraction time is 4 to 6 hours.

5. The preparation method of the flaxseed oil and hemp seed oil blended blend oil according to claim 2, characterized in that: the mass ratio of the added butyl hydroxy anisole to the total product is 0.010-0.015: 100.

6. The preparation method of the flaxseed oil and hemp seed oil blended blend oil according to claim 2, characterized in that: the solvent added in the process of preparing the tannin extracting solution is ethyl acetate.

7. The preparation method of the flaxseed oil and hemp seed oil blended blend oil according to claim 2, characterized in that: when the buffer solution is prepared, adding citric acid, and controlling the pH value to be 3-4.

Technical Field

The invention relates to the technical field of blend oil preparation, and particularly relates to a flaxseed oil and hemp seed oil blended blend oil and a preparation method thereof.

Background

The fructus cannabis contains edestin and edestin, the edestin is the most easily digested and absorbed by human body, and the edestin contains a large amount of arginine and methionine required by human body, and the linseed mainly contains unsaturated fatty acid, protein and mineral group, wherein the unsaturated fatty acid can be used as a main nutrient component to regulate blood fat, clear thrombus, participate in immune regulation, enhance immunity and the like.

The unsaturated fatty acid mainly comprises alpha-linolenic acid, the alpha-linolenic acid contains three unsaturated bonds, so that the chemical property of the alpha-linolenic acid is unstable and the alpha-linolenic acid can be oxidized in the air to form trans-linolenic acid, while other unsaturated fatty acids can generate trans-fatty acids which are harmful to human bodies, so that some auxiliary agents are required to be added to maintain the stability of nutritional ingredients, and the added auxiliary agents are nontoxic and harmless to the human bodies, so that the linseed oil and hemp seed oil blending and blending oil and the preparation method thereof are particularly important.

Disclosure of Invention

The invention aims to provide a flaxseed oil and hemp seed oil blended and compounded blend oil and a preparation method thereof, and aims to solve the problems in the background art.

In order to solve the technical problems, the invention provides the following technical scheme: the blended and compounded linseed oil and hemp seed oil comprises, by weight, 5-10 parts of linseed, 15-30 parts of hemp seed, 3-5 parts of nutgall powder and 0.4-0.5 part of sodium tripolyphosphate.

A preparation method of a flaxseed oil and hemp seed oil blended compound blend oil comprises the following steps,

(1) extracting Chinese gall powder:

adding deionized water into nutgall powder for leaching, filtering, decoloring, adding ethyl acetate, heating at the temperature of 40-50 ℃, stirring for 30-40 min, standing for layering to obtain a tannin extracting solution and a supernatant;

secondly, taking out the supernatant obtained in the first step, adding sulfuric acid at the temperature of 90-95 ℃, stirring for 30-40 min, adding diethyl ether and ethyl acetate, stirring, standing and layering to obtain a supernatant A and a supernatant A;

taking out the supernatant A obtained in the second step, drying, adding deionized water at the temperature of 70-80 ℃ for dissolving, and adding glucose hydrolase and catalase to obtain a gluconic acid extracting solution;

adding propanol and sulfuric acid into the supernate A obtained in the step two, stirring, filtering after complete reaction, adding ethanol for extraction, extracting for 3 times, centrifuging, and heating to obtain propyl gallate extracting solution;

(2) preparing flaxseed and hemp seed oil:

heating 1/3 sodium tripolyphosphate, adding citric acid, controlling the pH value to be 3-4 to obtain a buffer solution, dehulling flaxseeds, adding the buffer solution, stirring, and carrying out hot pressing to obtain flaxseed oil and residue A;

peeling hemp seeds, crushing, putting into an extraction tank, and performing subcritical butane extraction to obtain hemp seed oil and residue B;

mixing the residue A and the residue B, adding a tannin extracting solution, a gluconic acid extracting solution and a propyl gallate extracting solution, and extracting to obtain recovered nutritional ingredients;

and fourthly, mixing the linseed oil obtained in the step one and the hemp seed oil obtained in the step two, adding 2/3 sodium tripolyphosphate, stirring, adding the recovered nutritional ingredients obtained in the step three, mixing, stirring, centrifuging, decoloring and deodorizing, adding citric acid and butyl hydroxy anisole, heating, and removing organic solvents and enzymes to obtain the compound blend oil.

Further, the step of recovering the residue A and the residue B is as follows,

mixing the residue A and the residue B, adding ethanol and a tannin extracting solution, heating in a water bath at the temperature of 80-90 ℃, adding sodium hydroxide, extracting for 1-2 hours, and centrifuging to obtain a supernatant;

adding a gluconic acid extracting solution and a propyl gallate extracting solution into the supernatant obtained in the step one, adding sodium hydroxide, maintaining the pH value at 6-7, stirring, standing, adding ethanol, stirring, cooling, wherein the temperature is 3-5 ℃, and centrifuging to obtain recovered protein and waste liquid;

thirdly, adding barium chloride into the waste liquid, stirring, filtering, heating and drying, adding ethanol, stirring, filtering, drying, repeating for three times to obtain recovered protein, and mixing with the recovered protein obtained in the second step to obtain recovered nutrient components.

Further, when the hemp seeds are extracted, the pressure of an extraction tank is controlled to be-0.1 to-0.05 MPa, the extraction temperature is 60 to 70 ℃, the butane flow is 2 to 3L/min, and the extraction time is 4 to 6 hours.

Furthermore, the mass ratio of the added butyl hydroxy anisole to the total product is 0.010-0.015: 100.

Furthermore, the solvent added in the preparation of the tannin extract is ethyl acetate.

Further, when a buffer solution is prepared, after citric acid is added, the pH value is controlled to be 3-4.

Compared with the prior art, the invention has the following beneficial effects: the hemp seeds contain edestin and edestin, the edestin is the one most easily digested and absorbed by human body, and the edestin contains a large amount of arginine and methionine required by human body, the linseed mainly contains unsaturated fatty acid, protein and mineral group, in which the unsaturated fatty acid can be used as main nutrient component for regulating blood fat, cleaning thrombus and raising immunity, and the unsaturated fatty acid is mainly formed from alpha-linolenic acid, and the alpha-linolenic acid contains three unsaturated bonds, so that its chemical property is unstable, and can be oxidized in air to form trans-linolenic acid, and other unsaturated fatty acids can produce trans-fatty acid, and the production of trans-fatty acid can produce harm to human body, so that in the preparation process said invention adds antioxidant butyl hydroxy anisole and sodium tripolyphosphate, they can act synergistically as antioxidants to increase the antioxidant capacity of the product, reduce the production of trans fatty acids, increase the shelf life of the product and increase the content of nutritional ingredients.

The added butyl hydroxy anisole has certain toxicity and belongs to substances in a carcinogenic list, so that the invention selects more natural Chinese gall to replace partial butyl hydroxy anisole, reduces the harm to human bodies, extracts tannin in the Chinese magnoliavine fruit by extracting the Chinese magnoliavine fruit, not only can increase the nutritional variety of products, but also can improve the oxidation resistance of unsaturated fatty acid in the products. During secondary treatment of the hemp seed and linseed residues, tannin is added, so that the rate of residual protein precipitation can be increased, the recovery efficiency is improved, the generation of a by-product gallic acid can be increased under an acidic condition, and the oxidation resistance of the product can be increased by the gallic acid.

The gallic acid also can generate by-product glucose, and the glucose can be used as a nutrient component of most microorganisms to cause the growth of the microorganisms, so that the product is deteriorated and has suspended objects, and the quality guarantee period of the product is further reduced. And the generated gluconic acid can be used as an antioxidant to be matched with gallic acid ester, and can also adjust the pH value of the system, thereby ensuring the stability of the system. Since hydrogen peroxide is generated in the process of generating gluconic acid, catalase needs to be added to decompose the gluconic acid, so that the content of the hydrogen peroxide is reduced.

The preparation method comprises the steps of adding ethanol, filtering and drying, wherein sodium sulfate is generated in the preparation process, and the yield of the product can be reduced.

Detailed Description

The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Example 1

The blended oil comprises, by weight, 5 parts of flaxseed, 15 parts of fructus cannabis, 3 parts of nutgall powder and 0.4 part of sodium tripolyphosphate.

A preparation method of a flaxseed oil and hemp seed oil blended compound blend oil comprises the following steps,

(1) extracting Chinese gall powder:

adding deionized water into nutgall powder for leaching, filtering, decoloring, adding ethyl acetate, heating at 40 ℃, stirring for 30min, standing for layering to obtain tannin extracting solution and supernate;

② taking out the supernatant obtained in the step I, adding sulfuric acid at the temperature of 90 ℃, stirring for 30min, adding ether and ethyl acetate, stirring, standing and layering to obtain supernatant A and supernatant A;

taking out the supernatant A obtained in the second step, drying, adding deionized water at the temperature of 70 ℃ for dissolving, and adding glucose hydrolase and catalase to obtain a gluconic acid extracting solution;

adding propanol and sulfuric acid into the supernate A obtained in the step two, stirring, filtering after complete reaction, adding ethanol for extraction, extracting for 3 times, centrifuging, and heating to obtain propyl gallate extracting solution;

(2) preparing flaxseed and hemp seed oil:

heating 1/3 sodium tripolyphosphate, adding citric acid, controlling pH to 3 to obtain buffer solution, dehulling semen Lini, adding buffer solution, stirring, and hot pressing to obtain oleum Lini and residue A;

peeling hemp seeds, crushing, putting into an extraction tank, and performing subcritical butane extraction, wherein the pressure of the extraction tank is controlled at-0.1 MPa, the extraction temperature is 60 ℃, the butane flow is 2L/min, and the extraction time is 4h, so that hemp seed oil and residue B are obtained;

mixing the residue A and the residue B, adding ethanol and tannin extracting solution, heating in water bath at 80 ℃, adding sodium hydroxide, extracting for 1h, and centrifuging to obtain supernatant;

adding a gluconic acid extracting solution and a propyl gallate extracting solution into the supernatant obtained in the step (III), adding sodium hydroxide, maintaining the pH value to be 6, stirring, standing, adding ethanol, stirring, cooling, and centrifuging at the temperature of 3 ℃ to obtain recovered protein and waste liquid;

fifthly, adding barium chloride into the waste liquid, stirring, filtering, heating and drying, adding ethanol, stirring, filtering, drying, repeating for three times to obtain recovered protein, and mixing with the recovered protein obtained in the step IV to obtain recovered nutrient components;

sixthly, mixing the linseed oil obtained in the step I and the hemp seed oil obtained in the step II, adding 2/3 sodium tripolyphosphate, stirring, adding the recovered nutrient components obtained in the step II, mixing, stirring, centrifuging, decoloring and deodorizing, adding citric acid and butyl hydroxy anisole, heating the added butyl hydroxy anisole to remove the organic solvent and the enzyme, and obtaining the compound blend oil, wherein the mass ratio of the added butyl hydroxy anisole to the total product is 0.010: 100.

Example 2

The blended oil comprises, by weight, 5 parts of flaxseed, 15 parts of fructus cannabis, 3 parts of nutgall powder and 0.4 part of sodium tripolyphosphate.

A preparation method of a flaxseed oil and hemp seed oil blended compound blend oil comprises the following steps,

(1) extracting Chinese gall powder:

adding deionized water into nutgall powder for leaching, filtering, decoloring, adding ethyl acetate, heating at 45 ℃, stirring for 35min, standing for layering to obtain tannin extracting solution and supernate;

② taking out the supernatant obtained in the step I, adding sulfuric acid at the temperature of 93 ℃, stirring for 35min, adding ether and ethyl acetate, stirring, standing and layering to obtain supernatant A and supernatant A;

taking out the supernatant A obtained in the second step, drying, adding deionized water at 75 ℃ for dissolving, and adding glucose hydrolase and catalase to obtain a gluconic acid extracting solution;

adding propanol and sulfuric acid into the supernate A obtained in the step two, stirring, filtering after complete reaction, adding ethanol for extraction, extracting for 3 times, centrifuging, and heating to obtain propyl gallate extracting solution;

(2) preparing flaxseed and hemp seed oil:

heating 1/3 sodium tripolyphosphate, adding citric acid, controlling pH to 4 to obtain buffer solution, dehulling semen Lini, adding buffer solution, stirring, and hot pressing to obtain oleum Lini and residue A;

peeling hemp seeds, crushing, putting into an extraction tank, and performing subcritical butane extraction, wherein the pressure of the extraction tank is controlled at-0.03 MPa, the extraction temperature is 65 ℃, the butane flow is 2.5L/min, and the extraction time is 5 hours, so that hemp seed oil and residue B are obtained;

mixing the residue A and the residue B, adding ethanol and tannin extracting solution, heating in water bath at 85 ℃, adding sodium hydroxide, extracting for 1.5h, and centrifuging to obtain supernatant;

adding a gluconic acid extracting solution and a propyl gallate extracting solution into the supernatant obtained in the step (III), adding sodium hydroxide, maintaining the pH value to be 7, stirring, standing, adding ethanol, stirring, cooling, and centrifuging at the temperature of 4 ℃ to obtain recovered protein and waste liquid;

fifthly, adding barium chloride into the waste liquid, stirring, filtering, heating and drying, adding ethanol, stirring, filtering, drying, repeating for three times to obtain recovered protein, and mixing with the recovered protein obtained in the step IV to obtain recovered nutrient components;

sixthly, mixing the linseed oil obtained in the step I and the hemp seed oil obtained in the step II, adding 2/3 sodium tripolyphosphate, stirring, adding the recovered nutritional ingredients obtained in the step II, mixing, stirring, centrifuging, decoloring and deodorizing, adding citric acid and butyl hydroxy anisole, heating the added butyl hydroxy anisole to remove the organic solvent and the enzyme, and obtaining the compound blend oil, wherein the mass ratio of the added butyl hydroxy anisole to the total product is 0.013: 100.

Example 3

The blended oil comprises, by weight, 10 parts of flaxseed, 30 parts of fructus cannabis, 5 parts of nutgall powder and 0.5 part of sodium tripolyphosphate.

A preparation method of a flaxseed oil and hemp seed oil blended compound blend oil comprises the following steps,

(1) extracting Chinese gall powder:

adding deionized water into nutgall powder for leaching, filtering, decoloring, adding ethyl acetate, heating at 50 ℃, stirring for 40min, standing for layering to obtain tannin extracting solution and supernate;

② taking out the supernatant obtained in the step I, adding sulfuric acid at the temperature of 95 ℃, stirring for 40min, adding ether and ethyl acetate, stirring, standing and layering to obtain supernatant A and supernatant A;

taking out the supernatant A obtained in the second step, drying, adding deionized water at the temperature of 80 ℃ for dissolving, and adding glucose hydrolase and catalase to obtain a gluconic acid extracting solution;

adding propanol and sulfuric acid into the supernate A obtained in the step two, stirring, filtering after complete reaction, adding ethanol for extraction, extracting for 3 times, centrifuging, and heating to obtain propyl gallate extracting solution;

(2) preparing flaxseed and hemp seed oil:

heating 1/3 sodium tripolyphosphate, adding citric acid, controlling pH to 4 to obtain buffer solution, dehulling semen Lini, adding buffer solution, stirring, and hot pressing to obtain oleum Lini and residue A;

peeling hemp seeds, crushing, putting into an extraction tank, and performing subcritical butane extraction, wherein the pressure of the extraction tank is controlled at-0.05 MPa, the extraction temperature is 70 ℃, the butane flow is 3L/min, and the extraction time is 6h, so that hemp seed oil and residue B are obtained;

mixing the residue A and the residue B, adding ethanol and tannin extracting solution, heating in water bath at 90 ℃, adding sodium hydroxide, extracting for 2h, and centrifuging to obtain supernatant;

adding a gluconic acid extracting solution and a propyl gallate extracting solution into the supernatant obtained in the step (III), adding sodium hydroxide, maintaining the pH value to be 7, stirring, standing, adding ethanol, stirring, cooling, and centrifuging at the temperature of 5 ℃ to obtain recovered protein and waste liquid;

fifthly, adding barium chloride into the waste liquid, stirring, filtering, heating and drying, adding ethanol, stirring, filtering, drying, repeating for three times to obtain recovered protein, and mixing with the recovered protein obtained in the step IV to obtain recovered nutrient components;

sixthly, mixing the linseed oil obtained in the step I and the hemp seed oil obtained in the step II, adding 2/3 sodium tripolyphosphate, stirring, adding the recovered nutrient components obtained in the step III, mixing, stirring, centrifuging, decoloring and deodorizing, adding citric acid and butyl hydroxy anisole, heating the added butyl hydroxy anisole to be 0.015:100 of the total product mass, and removing the organic solvent and the enzyme to obtain the compound blend oil.

Comparative example 1

The blended oil comprises, by weight, 10 parts of flaxseed, 30 parts of fructus cannabis, 5 parts of nutgall powder, 0.5 part of sodium tripolyphosphate and 4 parts of disodium hydrogen phosphate.

A preparation method of a flaxseed oil and hemp seed oil blended compound blend oil comprises the following steps,

(1) extracting Chinese gall powder:

adding deionized water into nutgall powder for leaching, filtering, decoloring, adding ethyl acetate, heating at 50 ℃, stirring for 40min, standing for layering to obtain tannin extracting solution and supernate;

② taking out the supernatant obtained in the step I, adding sulfuric acid at the temperature of 95 ℃, stirring for 40min, adding ether and ethyl acetate, stirring, standing and layering to obtain supernatant A and supernatant A;

taking out the supernatant A obtained in the second step, drying, adding deionized water at the temperature of 80 ℃ for dissolving, and adding glucose hydrolase and catalase to obtain a gluconic acid extracting solution;

adding propanol and sulfuric acid into the supernate A obtained in the step two, stirring, filtering after complete reaction, adding ethanol for extraction, extracting for 3 times, centrifuging, and heating to obtain propyl gallate extracting solution;

(2) preparing flaxseed and hemp seed oil:

heating disodium hydrogen phosphate, adding citric acid, controlling the pH value to be 4 to obtain a buffer solution, dehulling flaxseeds, adding the buffer solution, stirring, and carrying out hot pressing to obtain flaxseed oil and residue A;

peeling hemp seeds, crushing, putting into an extraction tank, and performing subcritical butane extraction, wherein the pressure of the extraction tank is controlled at-0.05 MPa, the extraction temperature is 70 ℃, the butane flow is 3L/min, and the extraction time is 6h, so that hemp seed oil and residue B are obtained;

mixing the residue A and the residue B, adding ethanol and tannin extracting solution, heating in water bath at 90 ℃, adding sodium hydroxide, extracting for 2h, and centrifuging to obtain supernatant;

adding a gluconic acid extracting solution and a propyl gallate extracting solution into the supernatant obtained in the step (III), adding sodium hydroxide, maintaining the pH value to be 7, stirring, standing, adding ethanol, stirring, cooling, and centrifuging at the temperature of 5 ℃ to obtain recovered protein and waste liquid;

fifthly, adding barium chloride into the waste liquid, stirring, filtering, heating and drying, adding ethanol, stirring, filtering, drying, repeating for three times to obtain recovered protein, and mixing with the recovered protein obtained in the step IV to obtain recovered nutrient components;

sixthly, mixing the linseed oil obtained in the step I and the hemp seed oil obtained in the step II, adding sodium tripolyphosphate, stirring, adding the recovered nutritional ingredients obtained in the step II, mixing, stirring, centrifuging, decoloring and deodorizing, adding citric acid and butyl hydroxy anisole, adding the butyl hydroxy anisole at a mass ratio of 0.015:100 of the total product, heating, and removing the organic solvent and the enzyme to obtain the compound blend oil.

Comparative example 2

The blended oil comprises, by weight, 10 parts of flaxseed, 30 parts of fructus cannabis, 5 parts of nutgall powder and 0.5 part of sodium tripolyphosphate.

A preparation method of a flaxseed oil and hemp seed oil blended compound blend oil comprises the following steps,

(1) extracting Chinese gall powder:

adding acetone into the gallnut powder, carrying out ultrasonic treatment, collecting supernatant, adding chloroform, stirring, taking a water phase, adding ethyl acetate for extraction, oscillating, and drying to obtain tannin;

(2) preparing flaxseed and hemp seed oil:

heating 1/3 sodium tripolyphosphate, adding citric acid, controlling pH to 4 to obtain buffer solution, dehulling semen Lini, adding buffer solution, stirring, and hot pressing to obtain oleum Lini and residue A;

peeling hemp seeds, crushing, putting into an extraction tank, and performing subcritical butane extraction, wherein the pressure of the extraction tank is controlled at-0.05 MPa, the extraction temperature is 70 ℃, the butane flow is 3L/min, and the extraction time is 6h, so that hemp seed oil and residue B are obtained;

mixing the residue A and the residue B, adding ethanol, heating in water bath at 90 ℃, adding sodium hydroxide, extracting for 2h, and centrifuging to obtain a supernatant;

adding sodium hydroxide into the supernatant obtained in the step (III), maintaining the pH value to be 7, stirring, standing, adding ethanol, stirring, cooling to 5 ℃, and centrifuging to obtain recovered protein and waste liquid;

fifthly, adding barium chloride into the waste liquid, stirring, filtering, heating and drying, adding ethanol, stirring, filtering, drying, repeating for three times to obtain recovered protein, and mixing with the recovered protein obtained in the step IV to obtain recovered nutrient components;

sixthly, mixing the linseed oil obtained in the step I and the hemp seed oil obtained in the step II, adding 2/3 sodium tripolyphosphate, stirring, adding tannin and the recovered nutrient components obtained in the step III, mixing, stirring, centrifuging, decoloring and deodorizing, adding citric acid and butyl hydroxy anisole, heating the added butyl hydroxy anisole to the mass ratio of 0.015:100 of the total product, and removing the organic solvent and the enzyme to obtain the compound blend oil.

Comparative example 3

The blended oil comprises, by weight, 10 parts of flaxseed, 30 parts of fructus cannabis and 5 parts of nutgall powder.

A preparation method of a flaxseed oil and hemp seed oil blended compound blend oil comprises the following steps,

(1) extracting Chinese gall powder:

adding deionized water into nutgall powder for leaching, filtering, decoloring, adding ethyl acetate, heating at 50 ℃, stirring for 40min, standing for layering to obtain tannin extracting solution and supernate;

② taking out the supernatant obtained in the step I, adding sulfuric acid at the temperature of 95 ℃, stirring for 40min, adding ether and ethyl acetate, stirring, standing and layering to obtain supernatant A and supernatant A;

taking out the supernatant A obtained in the second step, drying, adding deionized water at the temperature of 80 ℃ for dissolving, and adding glucose hydrolase and catalase to obtain a gluconic acid extracting solution;

adding propanol and sulfuric acid into the supernate A obtained in the step two, stirring, filtering after complete reaction, adding ethanol for extraction, extracting for 3 times, centrifuging, and heating to obtain propyl gallate extracting solution;

(2) preparing flaxseed and hemp seed oil:

firstly, husking flaxseeds, stirring and carrying out hot pressing to obtain flaxseed oil and residue A;

peeling hemp seeds, crushing, putting into an extraction tank, and performing subcritical butane extraction, wherein the pressure of the extraction tank is controlled at-0.05 MPa, the extraction temperature is 70 ℃, the butane flow is 3L/min, and the extraction time is 6h, so that hemp seed oil and residue B are obtained;

mixing the residue A and the residue B, adding ethanol and tannin extracting solution, heating in water bath at 90 ℃, adding sodium hydroxide, extracting for 2h, and centrifuging to obtain supernatant;

adding a gluconic acid extracting solution and a propyl gallate extracting solution into the supernatant obtained in the step (III), adding sodium hydroxide, maintaining the pH value to be 7, stirring, standing, adding ethanol, stirring, cooling, and centrifuging at the temperature of 5 ℃ to obtain recovered protein and waste liquid;

fifthly, adding barium chloride into the waste liquid, stirring, filtering, heating and drying, adding ethanol, stirring, filtering, drying, repeating for three times to obtain recovered protein, and mixing with the recovered protein obtained in the step IV to obtain recovered nutrient components;

sixthly, mixing the linseed oil obtained in the step I and the hemp seed oil obtained in the step II, adding 2/3 sodium tripolyphosphate, stirring, adding the recovered nutrient components obtained in the step III, mixing, stirring, centrifuging, decoloring and deodorizing, adding citric acid and butyl hydroxy anisole, heating the added butyl hydroxy anisole to be 0.015:100 of the total product mass, and removing the organic solvent and the enzyme to obtain the compound blend oil.

Comparative example 4

The blended oil comprises, by weight, 10 parts of flaxseed, 30 parts of fructus cannabis, 5 parts of nutgall powder and 0.5 part of sodium tripolyphosphate.

A preparation method of a flaxseed oil and hemp seed oil blended compound blend oil comprises the following steps,

(1) extracting Chinese gall powder:

adding deionized water into nutgall powder for leaching, filtering, decoloring, adding ethyl acetate, heating at 50 ℃, stirring for 40min, standing for layering to obtain tannin extracting solution and supernate;

② taking out the supernatant obtained in the step I, adding sulfuric acid at the temperature of 95 ℃, stirring for 40min, adding ether and ethyl acetate, stirring, standing and layering to obtain a supernatant A;

thirdly, adding the propanol and the sulfuric acid into the supernatant A obtained in the second step, stirring, filtering after complete reaction, adding ethanol for extraction, extracting for 3 times, centrifuging, and heating to obtain propyl gallate extracting solution;

(2) preparing flaxseed and hemp seed oil:

heating 1/3 sodium tripolyphosphate, adding citric acid, controlling pH to 4 to obtain buffer solution, dehulling semen Lini, adding buffer solution, stirring, and hot pressing to obtain oleum Lini and residue A;

peeling hemp seeds, crushing, putting into an extraction tank, and performing subcritical butane extraction, wherein the pressure of the extraction tank is controlled at-0.05 MPa, the extraction temperature is 70 ℃, the butane flow is 3L/min, and the extraction time is 6h, so that hemp seed oil and residue B are obtained;

mixing the residue A and the residue B, adding ethanol and tannin extracting solution, heating in water bath at 90 ℃, adding sodium hydroxide, extracting for 2h, and centrifuging to obtain supernatant;

adding propyl gallate extracting solution into the supernatant obtained in the step (III), adding sodium hydroxide, maintaining the pH value at 7, stirring, standing, adding ethanol, stirring, cooling, keeping the temperature at 5 ℃, and centrifuging to obtain recovered protein and waste liquid;

fifthly, adding barium chloride into the waste liquid, stirring, filtering, heating and drying, adding ethanol, stirring, filtering, drying, repeating for three times to obtain recovered protein, and mixing with the recovered protein obtained in the step IV to obtain recovered nutrient components;

sixthly, mixing the linseed oil obtained in the step I and the hemp seed oil obtained in the step II, adding 2/3 sodium tripolyphosphate, stirring, adding the recovered nutrient components obtained in the step III, mixing, stirring, centrifuging, decoloring and deodorizing, adding citric acid and butyl hydroxy anisole, heating the added butyl hydroxy anisole to be 0.015:100 of the total product mass, and removing the organic solvent and the enzyme to obtain the compound blend oil.

Comparative example 5

The blended oil comprises, by weight, 10 parts of flaxseed, 30 parts of fructus cannabis, 5 parts of nutgall powder and 0.5 part of sodium tripolyphosphate.

A preparation method of a flaxseed oil and hemp seed oil blended compound blend oil comprises the following steps,

(1) extracting Chinese gall powder:

adding deionized water into nutgall powder for leaching, filtering, decoloring, adding ethyl acetate, heating at 50 ℃, stirring for 40min, standing for layering to obtain tannin extracting solution and supernate;

② taking out the supernatant obtained in the step I, adding sulfuric acid at the temperature of 95 ℃, stirring for 40min, adding ether and ethyl acetate, stirring, standing and layering to obtain supernatant A and supernatant A;

taking out the supernatant A obtained in the second step, drying, adding deionized water at the temperature of 80 ℃ for dissolving, and adding glucose hydrolase and catalase to obtain a gluconic acid extracting solution;

adding propanol and sulfuric acid into the supernate A obtained in the step two, stirring, filtering after complete reaction, adding ethanol for extraction, extracting for 3 times, centrifuging, and heating to obtain propyl gallate extracting solution;

(2) preparing flaxseed and hemp seed oil:

heating 1/3 sodium tripolyphosphate, adding citric acid, controlling pH to 4 to obtain buffer solution, dehulling semen Lini, adding buffer solution, stirring, and hot pressing to obtain oleum Lini and residue A;

peeling hemp seeds, crushing, putting into an extraction tank, and performing subcritical butane extraction, wherein the pressure of the extraction tank is controlled at-0.05 MPa, the extraction temperature is 70 ℃, the butane flow is 3L/min, and the extraction time is 6h, so that hemp seed oil and residue B are obtained;

mixing the residue A and the residue B, adding ethanol and tannin extracting solution, heating in water bath at 90 ℃, adding sodium hydroxide, extracting for 2h, and centrifuging to obtain supernatant;

adding a gluconic acid extracting solution and a propyl gallate extracting solution into the supernatant obtained in the step (III), adding sodium hydroxide, maintaining the pH value to be 7, stirring, standing, adding ethanol, stirring, cooling, and centrifuging at the temperature of 5 ℃ to obtain recovered protein;

fifthly, mixing the linseed oil obtained in the step I and the hemp seed oil obtained in the step II, adding 2/3 sodium tripolyphosphate, stirring, centrifuging, decoloring and deodorizing, adding citric acid and butyl hydroxy anisole, heating the mixture, and removing the organic solvent and the enzyme to obtain the compound blend oil, wherein the mass of the added butyl hydroxy anisole is 0.015:100 of that of the total product.

Experiment of

Taking example 3 as a control, a buffer solution is formed by adding disodium hydrogen phosphate and citric acid in comparative example 1, gallnut is extracted in one step in comparative example 2, no buffer solution is prepared in comparative example 3, no glucohydrolase is added in comparative example 4, and nutrient components in sodium sulfate raffinate are not recovered in comparative example 5.

The comparative experiments of example 1, example 2, example 3, comparative example 1, comparative example 2, comparative example 3, comparative example 4 and comparative example 5 were carried out, the content of butyl hydroxy anisole was measured according to the national standard GB 1886.12-2015, the content of phosphate was measured according to the national standard GB 5009.256-2016, and the results were as follows,

watch 1

Comparative experiments were conducted on example 1, example 2, example 3, comparative example 1, comparative example 2, comparative example 3, comparative example 4, and comparative example 5 to determine the peroxide value and the content of the essential nutrients in the product, and the results were as follows,

experimental group Peroxide number (g/100g) Essential nutrient substance
Example 1 0.07 92%
Example 2 0.05 91%
Example 3 0.07 90%
Comparative example 1 0.03 89%
Comparative example 2 0.09 84%
Comparative example 3 0.08 88%
Comparative example 4 0.13 83%
Comparative example 5 0.11 75%

Watch two

The contents of the butyl hydroxy anisole in the examples 1, 2, 3, 1, 2, 3 and 4 are all normal and meet the national index.

The peroxide number and the contents of main nutrients in comparative example 1 are better than those in examples 1, 2 and 3 because the buffer solution is formed by adding disodium hydrogen phosphate and citric acid in comparative example 1, the precipitation efficiency of nutrients can be improved, and the antioxidant capacity of the product can be enhanced by the disodium hydrogen phosphate, but the added disodium hydrogen phosphate is added independently, so that the total phosphate content in the system is high, and the product is unqualified.

The content of the main nutrient of comparative example 2 is inferior to that of examples 1, 2 and 3 because gallnut is extracted in one step in comparative example 2, tannin and gallic acid are not separated, and the content of the obtained protein is reduced, the content of the main nutrient is reduced, and the peroxidation value is higher than that of examples 1, 2 and 3, but the change range is smaller.

The content of the essential nutrients of comparative example 3 is inferior to that of examples 1, 2 and 3, and the peroxide value is the same as that of examples 1, 2 and 3, because no buffer solution is prepared in comparative example 3, resulting in incomplete precipitation of part of the nutrients when the residue is reprocessed, resulting in a decrease in the content of the essential nutrients.

The peroxide number and the contents of the main nutrients of comparative example 4 are inferior to those of examples 1, 2 and 3 in that no glucohydrolase is added to comparative example 4, resulting in a decrease in the oxidation resistance of the system and a decrease in the chelation of metals.

The peroxide number and the contents of the main nutrients in comparative example 5 are inferior to those of examples 1, 2 and 3 in that the nutrients in the sodium sulfate residual liquid are not recovered in comparative example 5, so that part of the nutrients are lost, and the performance of each aspect is reduced.

Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

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